CA1060627A - Arrangement for the sterilizing of a packing material web - Google Patents
Arrangement for the sterilizing of a packing material webInfo
- Publication number
- CA1060627A CA1060627A CA288,298A CA288298A CA1060627A CA 1060627 A CA1060627 A CA 1060627A CA 288298 A CA288298 A CA 288298A CA 1060627 A CA1060627 A CA 1060627A
- Authority
- CA
- Canada
- Prior art keywords
- sterilizing
- web
- sterilizing agent
- material web
- packing material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B55/00—Preserving, protecting or purifying packages or package contents in association with packaging
- B65B55/02—Sterilising, e.g. of complete packages
- B65B55/04—Sterilising wrappers or receptacles prior to, or during, packaging
- B65B55/10—Sterilising wrappers or receptacles prior to, or during, packaging by liquids or gases
- B65B55/103—Sterilising flat or tubular webs
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Apparatus For Disinfection Or Sterilisation (AREA)
- Containers And Plastic Fillers For Packaging (AREA)
- Packages (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
The present invention provides an arrangement for the sterilizing of a packing material web which in a packing machine is transformed to individual package units filled with sterile contents, which arrangement comprises units for the application of a liquid sterilizing agent to at least one side of the web and units for removing the sterilizing agent from the packing material web once the sterilizing effect has been achieved, the unit for the supply of sterilizing agent comprising a first treatment station with a container for sterilizing agent through which the packing material web is arranged to pass and with elements for the mechanical washing out of the packing material web, and a second treatment station comprising a chamber provided with inlet and outlet openings for the web, in which is arranged a nozzle element for directing sterilizing liquid towards a surface which is heatable to a temperature exceeding the temper-ature of evaporation of the sterilizing agent.
The present invention provides an arrangement for the sterilizing of a packing material web which in a packing machine is transformed to individual package units filled with sterile contents, which arrangement comprises units for the application of a liquid sterilizing agent to at least one side of the web and units for removing the sterilizing agent from the packing material web once the sterilizing effect has been achieved, the unit for the supply of sterilizing agent comprising a first treatment station with a container for sterilizing agent through which the packing material web is arranged to pass and with elements for the mechanical washing out of the packing material web, and a second treatment station comprising a chamber provided with inlet and outlet openings for the web, in which is arranged a nozzle element for directing sterilizing liquid towards a surface which is heatable to a temperature exceeding the temper-ature of evaporation of the sterilizing agent.
Description
iO606Z~7 The present invention relates to an arrangement for the ste-rilizing of a packing material web which in a packing machine is transformed to individual package units filled with sterile contents, which arrangement comprises units for the applica-tion of a liquid sterilizing agent to at least one side of the web as well as units~for removing the sterilizing agent again ~rom the pàcking material web once the sterilizing effect has been achieved.
A consumer package of the one-way type for e.g.
milk frequently encountered is manufactured from a web-shaped packing laminate comprising a carrier layer of fibrous mate-rial which is covered on either side with thin plastic layers.
The manufacture takes place in a known machine in such a manner that during the passage through the packing machine the web is folded to tube-shape in that both of its longitudinal edges are made to~o~erlap each other a little and are sealed to one an-- .. , . . , .................. : . - : ~ :
, . ~ , ; , , , ~, ~ ~ 6 ~7 other. This transPorming of the packing material web takes place continuously during the advance of the material web mainly vertically downwards through the machineO After the transformation to tube-shape, the contents are fed to the tube continuously through a filler pipe which extends into the tube through its upper open end. During the further ad-vance of the tube downwards, it is pressed flat and sealed by sealing jaws arranged on either side oP the tube along narrow transverse zones situated at a distance from one another. The supply of contents is controlled automatically during the whole time in such a manner that the level oP
contents is well above the point where the pressing flat and sealing of the tube take place. AÇter the sealing and possible shaping of the tube it is cut by transverse cuts in the sealing zones, whereupon the manufacture of the com-pletely filled individual packing units is complete.
The abovedescribed packing machine is known and it is also known that sterile packages can be manufactured on such a packing machine. Here the filling take,s place under aseptic conditions, which means that the atmosphere in the material tube as well as the material tube itself (or in any case its inside) have to be kept sterile. To achieve the former, a certain pressure of sterile air is maintained in the packing material tube, so that non-sterile air cannot penetrate in from the surrounding atmosphere. The steriliza-tion of the packing material web takes place in a known realization oP the machine described in that the packing material web, beore formation to tube-shape, is made to run through a bath o~ chemical sterilizing agent, usually a solu-tion of hydrogen peroxide, which is made to moisten the packing ~ -material, whereupon the excess liquid is stripped ofP the mate- :
rial web by means o mangle rollers. The portion of sterilizing agent which remains on *he packing material web is removed aPter th~ Pormation of the web to a tube Prom the inside oP the tube by means of a heating arrangement, usually a heating coil, a :
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so-called tube heater, arranged around the filler pipe which heats the inside of the packing material tube and the re-sidues of sterilizing agent remaining thereon to such an ex-tent that the agent is evaporated and escapes from the upper open end of the packing material tube. To ensure an even app-lication of sterilizing agent to the web, and hence an efPec-tive sterilization, the sterilizing agent has to contain a wetting agent which is a disadvantage, since the wetting agent cannot easily be fully removed and moreover implies an un-desirable extra cost.
Another method for providing sterilization of packing material webs in the type of machine described is also known. In accordance with this method a liquid steri-lizing agent, preferably a mixture of hydrogen peroxide and water, is introduced into a dishlike container present in the material tube. The container is situated around the filler pipe and is heated to such a temperature that the ste-rilizing agent when it is delivered dropwise to the dish eva-porates immediately. The vapour rises upwards through the tube and is deposited at the upper end o~ the inside wall of the tube. During the continuous movement downwards oP the tube the vapour, condensed at a certain moment at the upper end of the tube, will pass the tube heater of the type de-scribed earlier arranged in the tube which heats the inside wall of the tube as well as the sterilizing agent condensed on the same so vigorously that the agent is evaporated again and rises upwards to the region of the upper end o~ the tube where it is recondensed on the colder material wall.
This pro~ess is repeated as long as the packing machine is in operation, and the whole time a dropwise delivery of steri-lizing agent to the heated dish takes place, so as to replace the loss which arises through part of the evaporated steriliz-ing agent rising upwards through the upper end of the tube without being condensed on the tube wall.
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The sterilizing agent usually employed consists of hydrogen peroxide and water. The concentration of pure sterilizing agent in the mixture is only between 10-35% and cannot be increased appreciably since the risk of explosions of hydrogen peroxide increases with rising concentration.
When a drop of sterilizing agent mixture is delivered to the heated container the water portion will first escape in the form of steam, since the boiling point of hydrogen peroxide is appreciably higher than the boiling point of water. Only when the major part of the water in the drop has been eva-porated, the hydrogen peroxide in turn will operate which means therefore that the concentration of hydrogen peroxide inside the tube varies considerably, at the same rate as the delivery of drops of sterilisering agent. This is a disa~d-vantage which has been found to involve difficulties in the obtaining of a uniform sterilizing effect.
It is an object of the present invention to pro-vide an arrangement oP the type described in the beginning which ensures an effective sterilization without utilization of a wetting agent and without being subject to any of the disadvantages of the arrangements known hitherto.
These objects have been achie~ed in accordance with the invention through giving an arrangement of the type de- -scribed in-the introduction the characteristic that the unit for the supply of sterilizing agent comprises a first treat-ment station with a container ~or sterilizing liquid through which the packing material web is arranged to pass and with elements or the mechanical washing of the packing material web, and a second treatment station comprising a chamber pro-vided with inlet and outlet openings for the web in which is arranged a nozzle element Por sterilizing liquid which is ~-directed towards a surface which is heatable to a temperature exceeding the temperature oP evaporation of the sterilizing liquid used.
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06~7 A preferred embodiment oP the arrangement in accordance with the invention has been given moreover the characteristic that the heated surface is part of a heatable body and has a temperature o~ between ~60-250C.
The arrangement in accordance with the invention is further characterized in that the nozzle element is a spray nozzle.
It is a further characteristic of the arrangement in accordance with the invention that a time and pressure controlled valve is arranged upstream of the nozzle element so as to regulate the supply of sterilizing agent.
The invention will be described Purther in the following with re~erence to the enclosed drawing.
Fig. shows schematically and partly in cross-sectional presentation a preferred embodiment of the arrange-ment in accordance with the invention on a packing machine of known type.
Fig. 2 is a section through a part oP the arrange-ment in accordance with fig. 1.
The packing machine shown in fig. 1 manufactures individual liquid-filled packages from a continous packing material web 1 passing through the machine. The packing mate-rial web 1 is folded by the machine in an area designated by reference numeral 2 to a tubular body 3, which, aPter Pilling with sterile contents 4, is transversely sealed by means of seal-ing jaws-5 and cut to individual packages, not shown on the drawing. The machine comprises a number of guide rollers and other guide elements for the packing material web which, how-ever, are of the conventional type and in most cases are not shown on the drawing. During the transformation of the packing material web to tubular shape, the web i5 moved mainly ver-tically downwards from an upper pulley 6 to a forming ele-ment 7 which consists of a number of freely rotating rolls arranged in a~nular form. When the packing material web 1 has reached the forming element 7, the two longitudinal edges of - , .
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6 lO~ iiZ7 the web overlap one another a little, and with the help of a heating element 8 arranged directly above the forming ele-ment 7 the thermoplastic layer of the two edges is heated, whereupon the edges are pressed together with the help of a compression element 9, so that a longitudinal seal is formed.
Above the heating element 8 is located a pipe for the supply of sterile contents to the lower end of the tube 3 which is sealed so that it is impervious for liquids, where a float (not shown on the drawing) monitors the level of the contents and controls the delivery so that the level of contents is always above the level at which the transverse clamping together and sealing of the tube takes place by means of the jaws 5.
The filler pipe 10 is surrounded for the greater part o~
its length with a supply pipe 11 for sterile air. The supply pipe 11 extends vertically downwards through the tube 3 and ends at some distance above the contents level in a so-called jet deflector 12, which deflects the air flowing from the annular lower end of the supply pipe 11 so that the same is blown upwards through the tube 3. Beside the two supply pipes 10 and 11 for the contents and the sterile air respectively a tube heater,13 is present in the material tube 3 which con-sis'ts of an electrically heat'able element located co-axially around the two supply pipes.
The packing machine described which is known in itself compr~ses in accordance with the invention elements for the sterilization o~ the packing material web, more pre-cisely in the form of a first treatment station 14 and a second treatment station 15. The first treatment station 14 is situated at the upper end of the machine and comprises a container 16 for sterilizing liquid 17 and elements 18 for the wiping of the sterilizing agent from the web. In the lower part of the container a unit 19 is located comprising a guide roller around which the web is guided and a brush, sponge or the like arranged underneath the same which is ". . -~
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7 1~ ~0 ~'~7 rotatable and rests against the side of the web which sub-sequently will constitute the inside of the packing con-tainer. With the help of guide rollers 20 upstream and down-stream of the container 16 the web is passed down into the bath of sterilizing agent 17 along the one wall ~ the con-tainer 16 and upwards out of the bath along the other wall of the container, the web 1 passing,as it emerges ~rom the container, the wiping element 18 which may be constituted e.g. of rubber scrapers.
When the pacXing material web 1 has passed the roller 6 located at the upper end of the packing machine it comes into contact with the second treatment station 15 which comprises a treatment chamber 21 which extends vertically from an upper inlet end 22 arranged in the vicinity of the roller 6 to a lower outlet end arranged on the tube forming element 7. The lower half of the treatment chamber 21 has the form of a conventional casing 23 which on the tube-Porming element 7 rests tightly against the outside of the material tube 3 and for the rest comprises the sealing ele-ment 8 as well as the supply pipes 10, 11 for contents and sterile air respectively. In the central part of the treat-ment chamber 21 is located a heatable body 24 in the form of a horizontally arranged plate, against the upper side of which is directed a nozzle element 25. The nozzle element 25 is fitted to the wall of the casing 23 and is connected to a line 26 ex-tending outside the treatment chamber 21, whose end extend down into a container 27 for sterilizing liquid. The line is also proyided with a pump 28 for sterilizing liquid and a time-controlled valve 29 for the regulation of the liquid flow to the nozzle 25. The upp~r part of the treatment chamber 21 com-prises an elongated body 30, which can be heated, and which is prbvided with two longitudinal guide rails 31 which with the help of a packing element 32 are arranged to rest tightly against the two longitudinal edges of the material web 1. The treatment chamber 21 is thus shaped like a half moon (fig. 2) , 8 10~06Z~7 and is limited by the heatable body 30, the two guide rails 31 and the side of the material web 1 turned towards the body 30. The section ~hrough the treatment chamber 21 shown in fig. 2 is taken at a le~el a little above the nozzle element 25, at which level the formation of the material web 1 to tubular shape has gone relatively far. A corresponding sec-tion through the upper end of the treatment chamber 21 (that is to say directly below the end indicated by reference numeral 22) would show a material web 1 which has only been given a very slight curvature and a treatment chamber 21 of a corresponding shape. Finally there is an outlet pipe 33 at the upper end of the treatment chamber 21 for the sterile air mixture flowing upwards through the tube 3 and treatment chamber 21 which will be described in detail in the following.
As can be seen from the drawing, the one wall oP
the treatment chamber 21 (on the le~thand side on the drawing) consists permanently of the packing material web itself, whilst the other wall portion of the treatment chamber 21 consists in the upper part oP the treatment chamber of the heatable body 30 and in the lower part of the treatment chamber of the casing 23. Between the packing material web and the body 30 and casing 33 respectively are the afore-mentioned guide rails 31 which guide the packing material web 1 on its path downwards towards the forming ring 7 and at the same time ensure with the help of packing 32 a good seal against the edge region of the material web 1. The guide rails 31 also contribute to the transformation of the packing material web on its way from the roller 6, where - the cross-section oP the web is plane, to the forming ring 7, where the~web has a circular cross-section.
The packing material web 1 consists of laminated material and comprises layers of paper, aluminium foil and thermoplastic material. During operation the web is ~ed to the upper end of the machine via a number o~ guide rollers ~`~
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and pulleys to enter the container 16 with sterilizing liquid 17. The container 16 is of mainly triangular cross-section and the packing material web 1 passes over a pulley 20 down along one sidewall oP the container through the washing unit 19, arranged at the base of the container 16, and up along the oppo~ite wall o~ the container to pass through the element 18 for the mechanical wiping off of the sterilizing agent bePore the web is guided again via a further guide roller 20 to the guide wheel 6 arranged at the upper end of the packing machine. The unit 19 comprises fixed or movable sponges, scrapers, brushes or the like which wash at least one side of the web which will later constitute the inside of the packing container.
This first treatment serves not only for bringing the web into contact with the sterilizing liquid, but also, through the mechanical cleansing, washes out or at least detaches and disperses the bacteria which are present on the web, and in this manner prepares the web for the subsequent treatment with sterilizing agent.
After the preparatory treatment described, the main treatment of the packing material web 1 takes place at the second treatment station 15, that is to say in the treat-ment chamber 21 at the upper end 22 of which the packiny material web is introduced directly after it has passed the guide roller 6. From the guide roller 6 the web is guided in plane condition between the guide rails 21 arranged on the heatable body 30. During the successive movement downwards through the packing machine, the web is now transformed to tubular shape with the help of the guide rails and the forming element. During the whole time the edges oP the packing material web 1 rest tightly against the packings 32 of the guide rails 31 and with the help of the web 1, the heatable body 30 and the casing 23 the closed treatment chamber 21 is thus Pormed against which the side ,:
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of the packing material web, which is to form the inside o.
the packins container is exposed during the whole distan-e - from the inlet opening 22 until the material has been t:dn~-. formed to indivi.dual packages. Into the treatment chamber 21 is blown, as mentioned earlier, continuously a stream of sterile air via the pipe 11. The air escapes at the lower end of the material tube 3 and is deflected by means of the jet deflector 12 so that it flows upwards between the tube heater 13 and the inner wall of the material tube 3 and furhter upwards.through the chamber 21 past the nozzle 25.and out through the outlet pipe 33 at the upper end of the chamber.
Sterile air is blown in the whole time to such an extent that .-. a certain pressure is obtained inside the tube, which ensures a good seal between the packings 32 and the edge region of the packing material 1 and ensures moreo~er that the surrounding air cannot penetrate in through possible small leaks in the treatment chamber 21.
During operation sterilizing agent, usually hydrogen peroxide, is fed to the nozzle 25. The peroxide is pumped by means o~ the pump 28 from the container.27 and with the help of the time-controlled valve 29 a certain quantity of hydrogen peroxide is injected at certain inter-vals into the treatment chamber 21. The nozzle 25 through :
which the hydrogen peroxide is injected is a spray nozzleand thus atomizes the peroxide injected to a very high de-gree so that it meets in the form of a mist or very small droplets the heatable body 24 arranged in front of the nozzle 25, whose surface facing the nozzle has a tempera-ture oP 1~0-250C. This temperature is regulated as a func-tion, in the first place of the temperature of evaporation oP the sterilizing agent used, in the second place of the quantity of sterilizing agent supplied, and in the third .
place oP the mass oP the heatable body, in such a manner that the sterilizing agent supplied (e.g. hydrogen peroxi-de) at no time:can cool down the sur.face of the body to a .
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~ 7 temperature below the temperature of evaporation of thesterilizing agent. This means that every small drop-let of hydrogen peroxide when it makes contact with the surface is immediately evaporated, that is to say the proportion of pure peroxide in each droplet is eva-porated at the same time as the proportion of water, which means that a homogeneous mist or vapour of hydrogen peroxide and water is produced. With the help of the sterile air injected down into the tube-shaped material 3 the vapour formed is now guided gently upwards into the treatment chamber 21 between the inside of the material web 1 and the oblong body 30 which is heated to a temperature high enough for the vapour not to condense on the same. The packing material web, on the other hand, is largely at room temperature which means that the vapour condenses in a uniform layer on the surface of the material web facing the treatment chamber 21, which in fact has been exposed previously already in the first treatment station 14 to a washing out and a first treatment with sterilizing agent. Through the washing out a large part of the bacteria has been removed, and the remainder of the bacteria layer has, so to speak> been evened out or spread, as a result of which each separate bacteria can more easily be reached by peroxide vapour which of course not only condenses on the paper but also on the ~acteria themselves. This allows a very good bactericidal effect to be achievedO The excess or unused part of the peroxide vapour is passed together with the sterile hot air further upward and out throughthe pipe 33, from where it can be conducted e.g. to a condenser for cooling and recovery of the peroxide. When the material web 1 has passed the upper part of the treatment chamber 21, no further peroxide vapour is supplied to it, but the inside of the material web now only comes into contact with the sterile air which is in-troduced vi~ the pipe 11. This air, which is in fact heated .
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1~)t;0~ 7 when it passes upwards past the tube heater 13, causes a certain part of the condensed hydrogen peroxide to escape, and when the actual section of the material web has passed the form ring 7 and reaches the level of tube heater 13, the material web is heated to such an extent that the re-maining part of the hydrogen peroxide condensed on the in-side of the paper is heated and dried and accompanies the sterile air upwards through the material tube. The part of the material which has passed the tube heater is now steri-lized and may be Pilled with sterile contents 4 via the supply-pipe 10. Since the stream of sterile air blown in through the pipe 11 flows upwards continuously through the material tube 3 past the tube heater 13, it is assured that no bacteria can be entrained with the air down to the space below the tube heater 13, so that the sterility re-mains high.
Thanks to the combined arrangement in accordance with the invention, comprising a first treatment station which mechanically cleans and dries the web and a second treatment station in which the sterilizing agent is made to condense -on the web, a bactericidal ePfect is achieved which exceeds the bactericidal effect obtained when similar arrangements were used separately. This can be explained by the effect mentioned earlier, whereby as a result of the first immer-sion in sterilizing agent and subsequent mechanical wiping, the bacteria, so to speak, are thinned out in a uniform layer over the whole web, which appreciably enhances the ~ePPect of the subsequent vapour of sterilizing agent.
It has been found that a nozzle 25 which ato-mizes the liquid as highly as possible gives the best ePPect which, as explained earlier, i5 due to the Pact that the difference between the vapour which is produced at the beginning of the varpourization and that at the end of the vapourlzation will be the more noticeable the greater is , . .. .. . . . . ~ . . ..
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~O~;()f~Z7 the size of each individual droplet of sterilizing agent.
In the case of large drops, that is to say drops in the true sense of the word, a concentration of sterilizing agent in the earliest stage of evaporation of 5% has been measured whilst at the end of the evaporation as --good as pure sterilizing agent was vaporized. This gives rise to undesirable variations where the content of sterilizing agent in the vapour is concerned, and makes more difficult any regulation of the delivery of steri-lizing agent and the sterilizing effect.
Since only the vapour is used, droplet forma-tion is avoided, which means that the risk of explosions which exists when e.g. hydrogen peroxide is used as a sterilizing agent is diminished. The upper part of the treatment chamber 21 is filled all the time with vapour and the delivery of sterilizing agent via the nozzle 25 takes place at intervals which are regulated with the help of the time-controlled nozzle which is set as a function, above all, of the rate of movement of the material webO
Since all the sterilizing agent is applied at the upper end of the machine, the distance between the application station and the level of contents will be great which means that the drying and removal of steri-lizing agent can be carried out very effectively, so that the risk oP any entrainment of sterilizing agent into the contents i5 eliminated.
A further advantage of the arrangement in accordance with the invention is finally that the wetting agent,;which previously had to be mixed into the steri-lizing agent in order to obtain a uniform film of steri- -lizing agent on the web, is no longer required, either in the first treatment station 14 where the main purpose consists in fact in the mechanical wiping of the web or .
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~060~;Z7 in the second treatment station 15, where the application of sterilizing agent in any case will be uniform, since it takes place by condensation.
The sterilizing arrangement in accordance with the invention can of course also be used on packing machines oP a type different from that described above. Thus it is possible to use the sterilizing arrangement on the type of packing machines which operate with individual packing material blanks if these are attached to some form of transport belt in their passage through the sterilizing arrangement.
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A consumer package of the one-way type for e.g.
milk frequently encountered is manufactured from a web-shaped packing laminate comprising a carrier layer of fibrous mate-rial which is covered on either side with thin plastic layers.
The manufacture takes place in a known machine in such a manner that during the passage through the packing machine the web is folded to tube-shape in that both of its longitudinal edges are made to~o~erlap each other a little and are sealed to one an-- .. , . . , .................. : . - : ~ :
, . ~ , ; , , , ~, ~ ~ 6 ~7 other. This transPorming of the packing material web takes place continuously during the advance of the material web mainly vertically downwards through the machineO After the transformation to tube-shape, the contents are fed to the tube continuously through a filler pipe which extends into the tube through its upper open end. During the further ad-vance of the tube downwards, it is pressed flat and sealed by sealing jaws arranged on either side oP the tube along narrow transverse zones situated at a distance from one another. The supply of contents is controlled automatically during the whole time in such a manner that the level oP
contents is well above the point where the pressing flat and sealing of the tube take place. AÇter the sealing and possible shaping of the tube it is cut by transverse cuts in the sealing zones, whereupon the manufacture of the com-pletely filled individual packing units is complete.
The abovedescribed packing machine is known and it is also known that sterile packages can be manufactured on such a packing machine. Here the filling take,s place under aseptic conditions, which means that the atmosphere in the material tube as well as the material tube itself (or in any case its inside) have to be kept sterile. To achieve the former, a certain pressure of sterile air is maintained in the packing material tube, so that non-sterile air cannot penetrate in from the surrounding atmosphere. The steriliza-tion of the packing material web takes place in a known realization oP the machine described in that the packing material web, beore formation to tube-shape, is made to run through a bath o~ chemical sterilizing agent, usually a solu-tion of hydrogen peroxide, which is made to moisten the packing ~ -material, whereupon the excess liquid is stripped ofP the mate- :
rial web by means o mangle rollers. The portion of sterilizing agent which remains on *he packing material web is removed aPter th~ Pormation of the web to a tube Prom the inside oP the tube by means of a heating arrangement, usually a heating coil, a :
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so-called tube heater, arranged around the filler pipe which heats the inside of the packing material tube and the re-sidues of sterilizing agent remaining thereon to such an ex-tent that the agent is evaporated and escapes from the upper open end of the packing material tube. To ensure an even app-lication of sterilizing agent to the web, and hence an efPec-tive sterilization, the sterilizing agent has to contain a wetting agent which is a disadvantage, since the wetting agent cannot easily be fully removed and moreover implies an un-desirable extra cost.
Another method for providing sterilization of packing material webs in the type of machine described is also known. In accordance with this method a liquid steri-lizing agent, preferably a mixture of hydrogen peroxide and water, is introduced into a dishlike container present in the material tube. The container is situated around the filler pipe and is heated to such a temperature that the ste-rilizing agent when it is delivered dropwise to the dish eva-porates immediately. The vapour rises upwards through the tube and is deposited at the upper end o~ the inside wall of the tube. During the continuous movement downwards oP the tube the vapour, condensed at a certain moment at the upper end of the tube, will pass the tube heater of the type de-scribed earlier arranged in the tube which heats the inside wall of the tube as well as the sterilizing agent condensed on the same so vigorously that the agent is evaporated again and rises upwards to the region of the upper end o~ the tube where it is recondensed on the colder material wall.
This pro~ess is repeated as long as the packing machine is in operation, and the whole time a dropwise delivery of steri-lizing agent to the heated dish takes place, so as to replace the loss which arises through part of the evaporated steriliz-ing agent rising upwards through the upper end of the tube without being condensed on the tube wall.
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The sterilizing agent usually employed consists of hydrogen peroxide and water. The concentration of pure sterilizing agent in the mixture is only between 10-35% and cannot be increased appreciably since the risk of explosions of hydrogen peroxide increases with rising concentration.
When a drop of sterilizing agent mixture is delivered to the heated container the water portion will first escape in the form of steam, since the boiling point of hydrogen peroxide is appreciably higher than the boiling point of water. Only when the major part of the water in the drop has been eva-porated, the hydrogen peroxide in turn will operate which means therefore that the concentration of hydrogen peroxide inside the tube varies considerably, at the same rate as the delivery of drops of sterilisering agent. This is a disa~d-vantage which has been found to involve difficulties in the obtaining of a uniform sterilizing effect.
It is an object of the present invention to pro-vide an arrangement oP the type described in the beginning which ensures an effective sterilization without utilization of a wetting agent and without being subject to any of the disadvantages of the arrangements known hitherto.
These objects have been achie~ed in accordance with the invention through giving an arrangement of the type de- -scribed in-the introduction the characteristic that the unit for the supply of sterilizing agent comprises a first treat-ment station with a container ~or sterilizing liquid through which the packing material web is arranged to pass and with elements or the mechanical washing of the packing material web, and a second treatment station comprising a chamber pro-vided with inlet and outlet openings for the web in which is arranged a nozzle element Por sterilizing liquid which is ~-directed towards a surface which is heatable to a temperature exceeding the temperature oP evaporation of the sterilizing liquid used.
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06~7 A preferred embodiment oP the arrangement in accordance with the invention has been given moreover the characteristic that the heated surface is part of a heatable body and has a temperature o~ between ~60-250C.
The arrangement in accordance with the invention is further characterized in that the nozzle element is a spray nozzle.
It is a further characteristic of the arrangement in accordance with the invention that a time and pressure controlled valve is arranged upstream of the nozzle element so as to regulate the supply of sterilizing agent.
The invention will be described Purther in the following with re~erence to the enclosed drawing.
Fig. shows schematically and partly in cross-sectional presentation a preferred embodiment of the arrange-ment in accordance with the invention on a packing machine of known type.
Fig. 2 is a section through a part oP the arrange-ment in accordance with fig. 1.
The packing machine shown in fig. 1 manufactures individual liquid-filled packages from a continous packing material web 1 passing through the machine. The packing mate-rial web 1 is folded by the machine in an area designated by reference numeral 2 to a tubular body 3, which, aPter Pilling with sterile contents 4, is transversely sealed by means of seal-ing jaws-5 and cut to individual packages, not shown on the drawing. The machine comprises a number of guide rollers and other guide elements for the packing material web which, how-ever, are of the conventional type and in most cases are not shown on the drawing. During the transformation of the packing material web to tubular shape, the web i5 moved mainly ver-tically downwards from an upper pulley 6 to a forming ele-ment 7 which consists of a number of freely rotating rolls arranged in a~nular form. When the packing material web 1 has reached the forming element 7, the two longitudinal edges of - , .
,, ~ -, , .
.
6 lO~ iiZ7 the web overlap one another a little, and with the help of a heating element 8 arranged directly above the forming ele-ment 7 the thermoplastic layer of the two edges is heated, whereupon the edges are pressed together with the help of a compression element 9, so that a longitudinal seal is formed.
Above the heating element 8 is located a pipe for the supply of sterile contents to the lower end of the tube 3 which is sealed so that it is impervious for liquids, where a float (not shown on the drawing) monitors the level of the contents and controls the delivery so that the level of contents is always above the level at which the transverse clamping together and sealing of the tube takes place by means of the jaws 5.
The filler pipe 10 is surrounded for the greater part o~
its length with a supply pipe 11 for sterile air. The supply pipe 11 extends vertically downwards through the tube 3 and ends at some distance above the contents level in a so-called jet deflector 12, which deflects the air flowing from the annular lower end of the supply pipe 11 so that the same is blown upwards through the tube 3. Beside the two supply pipes 10 and 11 for the contents and the sterile air respectively a tube heater,13 is present in the material tube 3 which con-sis'ts of an electrically heat'able element located co-axially around the two supply pipes.
The packing machine described which is known in itself compr~ses in accordance with the invention elements for the sterilization o~ the packing material web, more pre-cisely in the form of a first treatment station 14 and a second treatment station 15. The first treatment station 14 is situated at the upper end of the machine and comprises a container 16 for sterilizing liquid 17 and elements 18 for the wiping of the sterilizing agent from the web. In the lower part of the container a unit 19 is located comprising a guide roller around which the web is guided and a brush, sponge or the like arranged underneath the same which is ". . -~
~, ~ . ..
. .
7 1~ ~0 ~'~7 rotatable and rests against the side of the web which sub-sequently will constitute the inside of the packing con-tainer. With the help of guide rollers 20 upstream and down-stream of the container 16 the web is passed down into the bath of sterilizing agent 17 along the one wall ~ the con-tainer 16 and upwards out of the bath along the other wall of the container, the web 1 passing,as it emerges ~rom the container, the wiping element 18 which may be constituted e.g. of rubber scrapers.
When the pacXing material web 1 has passed the roller 6 located at the upper end of the packing machine it comes into contact with the second treatment station 15 which comprises a treatment chamber 21 which extends vertically from an upper inlet end 22 arranged in the vicinity of the roller 6 to a lower outlet end arranged on the tube forming element 7. The lower half of the treatment chamber 21 has the form of a conventional casing 23 which on the tube-Porming element 7 rests tightly against the outside of the material tube 3 and for the rest comprises the sealing ele-ment 8 as well as the supply pipes 10, 11 for contents and sterile air respectively. In the central part of the treat-ment chamber 21 is located a heatable body 24 in the form of a horizontally arranged plate, against the upper side of which is directed a nozzle element 25. The nozzle element 25 is fitted to the wall of the casing 23 and is connected to a line 26 ex-tending outside the treatment chamber 21, whose end extend down into a container 27 for sterilizing liquid. The line is also proyided with a pump 28 for sterilizing liquid and a time-controlled valve 29 for the regulation of the liquid flow to the nozzle 25. The upp~r part of the treatment chamber 21 com-prises an elongated body 30, which can be heated, and which is prbvided with two longitudinal guide rails 31 which with the help of a packing element 32 are arranged to rest tightly against the two longitudinal edges of the material web 1. The treatment chamber 21 is thus shaped like a half moon (fig. 2) , 8 10~06Z~7 and is limited by the heatable body 30, the two guide rails 31 and the side of the material web 1 turned towards the body 30. The section ~hrough the treatment chamber 21 shown in fig. 2 is taken at a le~el a little above the nozzle element 25, at which level the formation of the material web 1 to tubular shape has gone relatively far. A corresponding sec-tion through the upper end of the treatment chamber 21 (that is to say directly below the end indicated by reference numeral 22) would show a material web 1 which has only been given a very slight curvature and a treatment chamber 21 of a corresponding shape. Finally there is an outlet pipe 33 at the upper end of the treatment chamber 21 for the sterile air mixture flowing upwards through the tube 3 and treatment chamber 21 which will be described in detail in the following.
As can be seen from the drawing, the one wall oP
the treatment chamber 21 (on the le~thand side on the drawing) consists permanently of the packing material web itself, whilst the other wall portion of the treatment chamber 21 consists in the upper part oP the treatment chamber of the heatable body 30 and in the lower part of the treatment chamber of the casing 23. Between the packing material web and the body 30 and casing 33 respectively are the afore-mentioned guide rails 31 which guide the packing material web 1 on its path downwards towards the forming ring 7 and at the same time ensure with the help of packing 32 a good seal against the edge region of the material web 1. The guide rails 31 also contribute to the transformation of the packing material web on its way from the roller 6, where - the cross-section oP the web is plane, to the forming ring 7, where the~web has a circular cross-section.
The packing material web 1 consists of laminated material and comprises layers of paper, aluminium foil and thermoplastic material. During operation the web is ~ed to the upper end of the machine via a number o~ guide rollers ~`~
~' 9 ~3~
and pulleys to enter the container 16 with sterilizing liquid 17. The container 16 is of mainly triangular cross-section and the packing material web 1 passes over a pulley 20 down along one sidewall oP the container through the washing unit 19, arranged at the base of the container 16, and up along the oppo~ite wall o~ the container to pass through the element 18 for the mechanical wiping off of the sterilizing agent bePore the web is guided again via a further guide roller 20 to the guide wheel 6 arranged at the upper end of the packing machine. The unit 19 comprises fixed or movable sponges, scrapers, brushes or the like which wash at least one side of the web which will later constitute the inside of the packing container.
This first treatment serves not only for bringing the web into contact with the sterilizing liquid, but also, through the mechanical cleansing, washes out or at least detaches and disperses the bacteria which are present on the web, and in this manner prepares the web for the subsequent treatment with sterilizing agent.
After the preparatory treatment described, the main treatment of the packing material web 1 takes place at the second treatment station 15, that is to say in the treat-ment chamber 21 at the upper end 22 of which the packiny material web is introduced directly after it has passed the guide roller 6. From the guide roller 6 the web is guided in plane condition between the guide rails 21 arranged on the heatable body 30. During the successive movement downwards through the packing machine, the web is now transformed to tubular shape with the help of the guide rails and the forming element. During the whole time the edges oP the packing material web 1 rest tightly against the packings 32 of the guide rails 31 and with the help of the web 1, the heatable body 30 and the casing 23 the closed treatment chamber 21 is thus Pormed against which the side ,:
:.
.` ~ .
, ;-- . :
. .
'~ i 10 .: - ~ .
of the packing material web, which is to form the inside o.
the packins container is exposed during the whole distan-e - from the inlet opening 22 until the material has been t:dn~-. formed to indivi.dual packages. Into the treatment chamber 21 is blown, as mentioned earlier, continuously a stream of sterile air via the pipe 11. The air escapes at the lower end of the material tube 3 and is deflected by means of the jet deflector 12 so that it flows upwards between the tube heater 13 and the inner wall of the material tube 3 and furhter upwards.through the chamber 21 past the nozzle 25.and out through the outlet pipe 33 at the upper end of the chamber.
Sterile air is blown in the whole time to such an extent that .-. a certain pressure is obtained inside the tube, which ensures a good seal between the packings 32 and the edge region of the packing material 1 and ensures moreo~er that the surrounding air cannot penetrate in through possible small leaks in the treatment chamber 21.
During operation sterilizing agent, usually hydrogen peroxide, is fed to the nozzle 25. The peroxide is pumped by means o~ the pump 28 from the container.27 and with the help of the time-controlled valve 29 a certain quantity of hydrogen peroxide is injected at certain inter-vals into the treatment chamber 21. The nozzle 25 through :
which the hydrogen peroxide is injected is a spray nozzleand thus atomizes the peroxide injected to a very high de-gree so that it meets in the form of a mist or very small droplets the heatable body 24 arranged in front of the nozzle 25, whose surface facing the nozzle has a tempera-ture oP 1~0-250C. This temperature is regulated as a func-tion, in the first place of the temperature of evaporation oP the sterilizing agent used, in the second place of the quantity of sterilizing agent supplied, and in the third .
place oP the mass oP the heatable body, in such a manner that the sterilizing agent supplied (e.g. hydrogen peroxi-de) at no time:can cool down the sur.face of the body to a .
.
.. . .
. ~ .
~ 7 temperature below the temperature of evaporation of thesterilizing agent. This means that every small drop-let of hydrogen peroxide when it makes contact with the surface is immediately evaporated, that is to say the proportion of pure peroxide in each droplet is eva-porated at the same time as the proportion of water, which means that a homogeneous mist or vapour of hydrogen peroxide and water is produced. With the help of the sterile air injected down into the tube-shaped material 3 the vapour formed is now guided gently upwards into the treatment chamber 21 between the inside of the material web 1 and the oblong body 30 which is heated to a temperature high enough for the vapour not to condense on the same. The packing material web, on the other hand, is largely at room temperature which means that the vapour condenses in a uniform layer on the surface of the material web facing the treatment chamber 21, which in fact has been exposed previously already in the first treatment station 14 to a washing out and a first treatment with sterilizing agent. Through the washing out a large part of the bacteria has been removed, and the remainder of the bacteria layer has, so to speak> been evened out or spread, as a result of which each separate bacteria can more easily be reached by peroxide vapour which of course not only condenses on the paper but also on the ~acteria themselves. This allows a very good bactericidal effect to be achievedO The excess or unused part of the peroxide vapour is passed together with the sterile hot air further upward and out throughthe pipe 33, from where it can be conducted e.g. to a condenser for cooling and recovery of the peroxide. When the material web 1 has passed the upper part of the treatment chamber 21, no further peroxide vapour is supplied to it, but the inside of the material web now only comes into contact with the sterile air which is in-troduced vi~ the pipe 11. This air, which is in fact heated .
,, . . - : . . , , ~ .: , . . .
1~)t;0~ 7 when it passes upwards past the tube heater 13, causes a certain part of the condensed hydrogen peroxide to escape, and when the actual section of the material web has passed the form ring 7 and reaches the level of tube heater 13, the material web is heated to such an extent that the re-maining part of the hydrogen peroxide condensed on the in-side of the paper is heated and dried and accompanies the sterile air upwards through the material tube. The part of the material which has passed the tube heater is now steri-lized and may be Pilled with sterile contents 4 via the supply-pipe 10. Since the stream of sterile air blown in through the pipe 11 flows upwards continuously through the material tube 3 past the tube heater 13, it is assured that no bacteria can be entrained with the air down to the space below the tube heater 13, so that the sterility re-mains high.
Thanks to the combined arrangement in accordance with the invention, comprising a first treatment station which mechanically cleans and dries the web and a second treatment station in which the sterilizing agent is made to condense -on the web, a bactericidal ePfect is achieved which exceeds the bactericidal effect obtained when similar arrangements were used separately. This can be explained by the effect mentioned earlier, whereby as a result of the first immer-sion in sterilizing agent and subsequent mechanical wiping, the bacteria, so to speak, are thinned out in a uniform layer over the whole web, which appreciably enhances the ~ePPect of the subsequent vapour of sterilizing agent.
It has been found that a nozzle 25 which ato-mizes the liquid as highly as possible gives the best ePPect which, as explained earlier, i5 due to the Pact that the difference between the vapour which is produced at the beginning of the varpourization and that at the end of the vapourlzation will be the more noticeable the greater is , . .. .. . . . . ~ . . ..
, . . . .. ,: . . . - .. : . :, . .. , . .. . : . . .
- ...... .. .
,; . . .
~O~;()f~Z7 the size of each individual droplet of sterilizing agent.
In the case of large drops, that is to say drops in the true sense of the word, a concentration of sterilizing agent in the earliest stage of evaporation of 5% has been measured whilst at the end of the evaporation as --good as pure sterilizing agent was vaporized. This gives rise to undesirable variations where the content of sterilizing agent in the vapour is concerned, and makes more difficult any regulation of the delivery of steri-lizing agent and the sterilizing effect.
Since only the vapour is used, droplet forma-tion is avoided, which means that the risk of explosions which exists when e.g. hydrogen peroxide is used as a sterilizing agent is diminished. The upper part of the treatment chamber 21 is filled all the time with vapour and the delivery of sterilizing agent via the nozzle 25 takes place at intervals which are regulated with the help of the time-controlled nozzle which is set as a function, above all, of the rate of movement of the material webO
Since all the sterilizing agent is applied at the upper end of the machine, the distance between the application station and the level of contents will be great which means that the drying and removal of steri-lizing agent can be carried out very effectively, so that the risk oP any entrainment of sterilizing agent into the contents i5 eliminated.
A further advantage of the arrangement in accordance with the invention is finally that the wetting agent,;which previously had to be mixed into the steri-lizing agent in order to obtain a uniform film of steri- -lizing agent on the web, is no longer required, either in the first treatment station 14 where the main purpose consists in fact in the mechanical wiping of the web or .
':
~060~;Z7 in the second treatment station 15, where the application of sterilizing agent in any case will be uniform, since it takes place by condensation.
The sterilizing arrangement in accordance with the invention can of course also be used on packing machines oP a type different from that described above. Thus it is possible to use the sterilizing arrangement on the type of packing machines which operate with individual packing material blanks if these are attached to some form of transport belt in their passage through the sterilizing arrangement.
.
.
" , ' ~
..
, . ~
Claims (4)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. An arrangement for the sterilizing of a packing material web which in a packing machine is transformed to individual package units filled with sterile contents, which arrangement comprises units for the application of a liquid sterilizing agent to at least one side of the web and units for removing the sterilizing agent from the packing material web once the sterilizing effect has been achieved, the unit for the supply of sterilizing agent comprising a first treatment station with a container for sterilizing agent through which the packing material web is arranged to pass and with elements for the mechanical washing out of the packing material web, and a second treatment station comprising a chamber provided with inlet and outlet openings for the web, in which is arranged a nozzle element for directing sterilizing liquid towards a surface which is heatable to a temperature exceeding the temper-ature of evaporation of the sterilizing agent.
2. An arrangement in accordance with claim 1, in which the heated surface forms part of a heatable body, said surface being adapted to be heated to a temperature of between 160-250°C.
3. An arrangement in accordance with claim 1, in which the nozzle element is a spray nozzle.
4. An arrangement in accordance with claim 1, 2 or 3, in which a time-controlled valve is arranged upstream of the nozzle element so as to regulate the supply of sterilizing agent.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE7611124A SE401913B (en) | 1976-10-07 | 1976-10-07 | DEVICE FOR STERILIZING A PACKAGING MATERIAL PATH |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1060627A true CA1060627A (en) | 1979-08-21 |
Family
ID=20329065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA288,298A Expired CA1060627A (en) | 1976-10-07 | 1977-10-07 | Arrangement for the sterilizing of a packing material web |
Country Status (12)
| Country | Link |
|---|---|
| US (1) | US4225556A (en) |
| JP (1) | JPS5346197A (en) |
| AU (1) | AU515476B2 (en) |
| CA (1) | CA1060627A (en) |
| CH (1) | CH621741A5 (en) |
| DE (1) | DE2744638C3 (en) |
| FR (1) | FR2366997A1 (en) |
| GB (1) | GB1574488A (en) |
| IT (1) | IT1088084B (en) |
| NL (1) | NL186234C (en) |
| SE (1) | SE401913B (en) |
| SU (1) | SU1258312A3 (en) |
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| JPS5675158A (en) * | 1979-11-27 | 1981-06-22 | Dainippon Printing Co Ltd | Sterilizer |
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| DE3235476C2 (en) * | 1981-11-14 | 1986-09-11 | Jagenberg AG, 4000 Düsseldorf | Method and device for disinfecting packaging material, in particular packaging containers |
| BE894957A (en) * | 1981-11-14 | 1983-03-01 | Jagenberg Ag | METHOD AND DEVICE FOR STERILIZING PACKAGING MATERIAL, IN PARTICULAR, PACKAGING CONTAINERS |
| GB2127692A (en) * | 1982-09-29 | 1984-04-18 | American Sterilizer Co | Hydrogen peroxide liquid film sterilization method |
| SE8405557D0 (en) * | 1983-11-07 | 1984-11-06 | American Sterilizer Co | SET CONCENTRATE VETEPEROXIDE |
| JPS60176762A (en) * | 1984-02-23 | 1985-09-10 | Idec Izumi Corp | Alighnment-discharge device for three dimensional product printer |
| DE3422683A1 (en) * | 1984-06-19 | 1985-12-19 | Tetra Pak Research GmbH, 7000 Stuttgart | METHOD FOR STERILIZING PACKAGING MATERIALS FOR ASEPTICALLY FILLING FRUIT JUICE AND WINE |
| AU592461B2 (en) * | 1986-06-26 | 1990-01-11 | Baxter International Inc. | Device for continuously cleaning and/or decontaminating a band of a thermoplastic film |
| US4909999A (en) * | 1987-07-06 | 1990-03-20 | American Sterilizer Company | Flow-through vapor phase sterilization system |
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| US4952370A (en) * | 1988-05-06 | 1990-08-28 | American Sterilizer Company | Hydrogen peroxide sterilization method |
| SE461264B (en) * | 1988-05-31 | 1990-01-29 | Roby Teknik Ab | SETTING AND DEVICE TO PROCESS A CURRENT MATERIAL RANGE |
| US5135714A (en) * | 1990-03-08 | 1992-08-04 | Fmc Corporation | Process for sterilizing a web of packaging material |
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| SE468982B (en) * | 1991-07-17 | 1993-04-26 | Tetra Alfa Holdings | SETTING AND DEVICE STERILIZING AND DRYING A CONTINUOUS PACKAGING MATERIAL WITH CURRENT WATER-PEROXIDE-CONTAINING AIR |
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| ATE216599T1 (en) * | 1997-10-29 | 2002-05-15 | Tetra Laval Holdings & Finance | METHOD AND DEVICE FOR STERILIZING PACKAGING MATERIAL SHEETS |
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| US6451254B1 (en) * | 1998-12-30 | 2002-09-17 | Ethicon, Inc. | Sterilization of diffusion-restricted area by revaporizing the condensed vapor |
| EP1050467B1 (en) | 1999-05-03 | 2004-03-03 | Tetra Laval Holdings & Finance SA | Unit for sterilizing strip material on a packaging machine for packaging pourable food products, and packaging machine comprising such a unit |
| DE69915594T2 (en) | 1999-05-03 | 2005-02-03 | Tetra Laval Holdings & Finance S.A. | Unit for sterilizing a material web in a packaging machine for packaging flowable food, and packaging machine with such a unit |
| US6354062B1 (en) | 1999-05-13 | 2002-03-12 | Bevtek Inc. | Method of manufacture of individual beverage carton with a straw therein |
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| CN105814138B (en) | 2013-11-22 | 2018-06-01 | 盛禧奥欧洲有限责任公司 | Composition containing makrolon |
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| CH537306A (en) * | 1971-07-09 | 1973-05-31 | Alpura Koreco Ag | Method and device for sterilizing the outside of a filling tube in aseptically operating packaging machines |
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-
1976
- 1976-10-07 SE SE7611124A patent/SE401913B/en not_active IP Right Cessation
-
1977
- 1977-09-29 GB GB40575/77A patent/GB1574488A/en not_active Expired
- 1977-10-04 NL NLAANVRAGE7710884,A patent/NL186234C/en not_active IP Right Cessation
- 1977-10-04 DE DE2744638A patent/DE2744638C3/en not_active Expired
- 1977-10-04 US US05/839,274 patent/US4225556A/en not_active Expired - Lifetime
- 1977-10-04 FR FR7729749A patent/FR2366997A1/en active Granted
- 1977-10-06 AU AU29434/77A patent/AU515476B2/en not_active Expired
- 1977-10-06 CH CH1225577A patent/CH621741A5/de not_active IP Right Cessation
- 1977-10-07 IT IT28383/77A patent/IT1088084B/en active
- 1977-10-07 JP JP12084577A patent/JPS5346197A/en active Granted
- 1977-10-07 SU SU2532453A patent/SU1258312A3/en active
- 1977-10-07 CA CA288,298A patent/CA1060627A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| IT1088084B (en) | 1985-06-04 |
| FR2366997B1 (en) | 1984-04-20 |
| CH621741A5 (en) | 1981-02-27 |
| JPS5729336B2 (en) | 1982-06-22 |
| SE401913B (en) | 1978-06-05 |
| DE2744638B2 (en) | 1979-08-02 |
| SU1258312A3 (en) | 1986-09-15 |
| FR2366997A1 (en) | 1978-05-05 |
| NL7710884A (en) | 1978-04-11 |
| US4225556A (en) | 1980-09-30 |
| AU2943477A (en) | 1979-04-12 |
| DE2744638A1 (en) | 1978-04-13 |
| DE2744638C3 (en) | 1980-04-17 |
| NL186234B (en) | 1990-05-16 |
| GB1574488A (en) | 1980-09-10 |
| NL186234C (en) | 1990-10-16 |
| AU515476B2 (en) | 1981-04-09 |
| SE7611124L (en) | 1978-04-08 |
| JPS5346197A (en) | 1978-04-25 |
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